Supplementary Material (ESI) for Journal of Materials Chemistry
This journal is © The Royal Society of Chemistry 2001

data_I
_database_code_CSD                  170511
_journal_coden_Cambridge            1145

_audit_creation_date            2001-10-18T20:08:31-00:00
_audit_creation_method         'WinGX routine CIF_UPDATE'
_chemical_name_systematic
;
Bis-tetramethylammonium-tri-zinc-tetra-hydrogenphosphate
;
_chemical_formula_sum                   'C8 H28 N2 O16 P4 Zn3'
_chemical_formula_weight                728.32
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'C'  'C'   0.0033   0.0016
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'H'  'H'   0.0000   0.0000
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'N'  'N'   0.0061   0.0033
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'O'  'O'   0.0106   0.0060
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'P'  'P'   0.1023   0.0942
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Zn'  'Zn'   0.2839   1.4301
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting                  orthorhombic
_symmetry_space_group_name_H-M          'F d d d'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/4, -y+1/4, z'
'x, -y+1/4, -z+1/4'
'-x+1/4, y, -z+1/4'
'x, y+1/2, z+1/2'
'-x+1/4, -y+3/4, z+1/2'
'x, -y+3/4, -z+3/4'
'-x+1/4, y+1/2, -z+3/4'
'x+1/2, y, z+1/2'
'-x+3/4, -y+1/4, z+1/2'
'x+1/2, -y+1/4, -z+3/4'
'-x+3/4, y, -z+3/4'
'x+1/2, y+1/2, z'
'-x+3/4, -y+3/4, z'
'x+1/2, -y+3/4, -z+1/4'
'-x+3/4, y+1/2, -z+1/4'
'-x, -y, -z'
'x-1/4, y-1/4, -z'
'-x, y-1/4, z-1/4'
'x-1/4, -y, z-1/4'
'-x, -y+1/2, -z+1/2'
'x-1/4, y+1/4, -z+1/2'
'-x, y+1/4, z+1/4'
'x-1/4, -y+1/2, z+1/4'
'-x+1/2, -y, -z+1/2'
'x+1/4, y-1/4, -z+1/2'
'-x+1/2, y-1/4, z+1/4'
'x+1/4, -y, z+1/4'
'-x+1/2, -y+1/2, -z'
'x+1/4, y+1/4, -z'
'-x+1/2, y+1/4, z-1/4'
'x+1/4, -y+1/2, z-1/4'
_cell_length_a                    9.203(1)
_cell_length_b                    15.776(2)
_cell_length_c                    31.587(4)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 90.00
_cell_volume                      4586(1)
_cell_formula_units_Z             8
_cell_measurement_temperature     293
_cell_measurement_reflns_used	        25
_cell_measurement_theta_min             10.49             
_cell_mesaurement_theta_max             14.54
_exptl_crystal_density_diffrn           2.110
_exptl_crystal_density_method           'not measured'
_exptl_crystal_F_000              2944
_exptl_crystal_description              'irregular plate'
_exptl_crystal_size_max                 0.22
_exptl_crystal_size_mid                 0.21
_exptl_crystal_size_min                 0.16
_exptl_crystal_colour			white
_exptl_special_details
;
?
;
_exptl_absorpt_coefficient_mu           3.469
_exptl_absorpt_correction_type          psi-scan
_exptl_absorpt_process_details
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
;
_exptl_absorpt_correction_T_min      	0.4198
_exptl_absorpt_correction_T_max      	0.4980
_exptl_absorpt_correction_T_ave      	0.4508
_diffrn_ambient_temperature             293
_diffrn_measurement_device_type         'Enraf Nonius CAD4'
_diffrn_measurement_method              '\w/2\Q-scan'
_diffrn_radiation_wavelength            0.71073
_diffrn_radiation_type                  MoK\a
_diffrn_radiation_monochromator         graphite
_diffrn_reflns_number                   3519
_diffrn_reflns_av_R_equivalents   0.0560
_diffrn_reflns_limit_h_min        0
_diffrn_reflns_limit_h_max        12
_diffrn_reflns_limit_k_min        -22
_diffrn_reflns_limit_k_max        0
_diffrn_reflns_limit_l_min        -44
_diffrn_reflns_limit_l_max        44
_diffrn_reflns_theta_min          2.58
_diffrn_reflns_theta_max          29.95
_diffrn_reflns_theta_full               29.95
_diffrn_measured_fraction_theta_full
1
_diffrn_measured_fraction_theta_max
1
_reflns_number_total              1668
_reflns_number_gt                 1040
_reflns_threshold_expression      >2sigma(I)
_computing_structure_solution           'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement         'SHELXL-97 (Sheldrick, 1997)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef        Fsqd
_refine_ls_matrix_type                  full
_refine_ls_weighting_scheme             calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0330P)^2^+10.5839P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    'geom difmap'
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          1668
_refine_ls_number_parameters      83
_refine_ls_number_restraints      2
_refine_ls_R_factor_all           0.0939
_refine_ls_R_factor_gt            0.0368
_refine_ls_wR_factor_ref          0.0868
_refine_ls_wR_factor_gt           0.0729
_refine_ls_goodness_of_fit_ref    1.020
_refine_ls_restrained_S_all       1.019
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
_refine_diff_density_max    0.933
_refine_diff_density_min   -0.548
_refine_diff_density_rms    0.131
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn -0.1250 0.3750 0.3750 0.0182(2) Uani 1 4 d S . .
Zn2 Zn -0.1250 0.3750 0.239279(17) 0.01834(16) Uani 1 2 d S . .
P P 0.10185(10) 0.30470(6) 0.30866(3) 0.01598(19) Uani 1 1 d . . .
O1 O 0.0525(3) 0.35630(18) 0.27112(9) 0.0284(7) Uani 1 1 d . . .
O2 O -0.0128(3) 0.29435(17) 0.34228(9) 0.0287(7) Uani 1 1 d . . .
O3 O 0.1713(3) 0.22186(17) 0.29649(8) 0.0279(7) Uani 1 1 d . . .
O4 O 0.2279(3) 0.3593(2) 0.33108(9) 0.0317(7) Uani 1 1 d D . .
H1 H 0.319(4) 0.359(7) 0.321(3) 0.050 Uiso 0.50 1 d PD . .
H2 H 0.181(9) 0.355(7) 0.3557(16) 0.050 Uiso 0.50 1 d PD . .
N N 0.3750 0.3750 0.18413(15) 0.0281(10) Uani 1 2 d S . .
C1 C 0.2501(10) 0.3932(8) 0.1593(3) 0.169(5) Uani 1 1 d . . .
H1A H 0.2259 0.3433 0.1416 0.203 Uiso 1 1 calc R . .
H1B H 0.2703 0.4424 0.1408 0.203 Uiso 1 1 calc R . .
H1C H 0.1673 0.4065 0.1781 0.203 Uiso 1 1 calc R . .
C2 C 0.3487(14) 0.3026(5) 0.2091(3) 0.199(7) Uani 1 1 d . . .
H2A H 0.3292 0.2535 0.1905 0.239 Uiso 1 1 calc R . .
H2B H 0.2635 0.3129 0.2276 0.239 Uiso 1 1 calc R . .
H2C H 0.4350 0.2908 0.2269 0.239 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zn1 0.0171(5) 0.0221(4) 0.0154(4) 0.000 0.000 0.000
Zn2 0.0237(3) 0.0155(3) 0.0157(3) 0.000 0.000 0.0051(3)
P 0.0169(4) 0.0156(4) 0.0154(4) -0.0029(3) -0.0017(4) 0.0024(3)
O1 0.0276(16) 0.0286(16) 0.0289(14) 0.0078(12) -0.0069(12) 0.0044(12)
O2 0.0300(16) 0.0258(15) 0.0304(15) -0.0034(13) 0.0094(13) 0.0013(13)
O3 0.0321(16) 0.0230(14) 0.0285(15) -0.0100(12) -0.0009(12) 0.0081(12)
O4 0.0235(16) 0.0351(19) 0.0365(17) -0.0116(13) -0.0048(13) -0.0056(14)
N 0.033(3) 0.025(2) 0.027(2) 0.000 0.000 -0.004(2)
C1 0.100(8) 0.191(13) 0.216(12) -0.029(11) -0.082(9) 0.011(8)
C2 0.296(16) 0.078(6) 0.222(11) 0.083(7) 0.193(12) 0.029(8)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix.  The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O2 1.937(3) 12_455 ?
Zn1 O2 1.937(3) 7 ?
Zn1 O2 1.937(3) . ?
Zn1 O2 1.937(3) 14_455 ?
Zn2 O1 1.941(3) . ?
Zn2 O1 1.941(3) 14_455 ?
Zn2 O3 1.948(3) 21 ?
Zn2 O3 1.948(3) 22 ?
P O3 1.505(3) . ?
P O2 1.506(3) . ?
P O1 1.509(3) . ?
P O4 1.609(3) . ?
O3 Zn2 1.948(3) 21 ?
N C2 1.409(7) 14 ?
N C2 1.409(7) . ?
N C1 1.421(8) . ?
N C1 1.421(8) 14 ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Zn1 O2 115.53(17) 12_455 7 ?
O2 Zn1 O2 97.90(17) 12_455 . ?
O2 Zn1 O2 115.57(18) 7 . ?
O2 Zn1 O2 115.57(18) 12_455 14_455 ?
O2 Zn1 O2 97.90(17) 7 14_455 ?
O2 Zn1 O2 115.53(17) . 14_455 ?
O1 Zn2 O1 117.58(17) . 14_455 ?
O1 Zn2 O3 111.44(12) . 21 ?
O1 Zn2 O3 103.63(12) 14_455 21 ?
O1 Zn2 O3 103.63(12) . 22 ?
O1 Zn2 O3 111.44(12) 14_455 22 ?
O3 Zn2 O3 109.08(17) 21 22 ?
O3 P O2 112.56(16) . . ?
O3 P O1 113.31(16) . . ?
O2 P O1 113.70(17) . . ?
O3 P O4 105.71(16) . . ?
O2 P O4 104.65(16) . . ?
O1 P O4 105.93(17) . . ?
P O1 Zn2 137.98(19) . . ?
P O2 Zn1 132.72(17) . . ?
P O3 Zn2 137.44(18) . 21 ?
C2 N C2 111.8(10) 14 . ?
C2 N C1 106.6(6) 14 . ?
C2 N C1 109.6(7) . . ?
C2 N C1 109.6(7) 14 14 ?
C2 N C1 106.6(6) . 14 ?
C1 N C1 112.9(9) . 14 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O4 H1 O4 . . 14555 0.90 1.96 2.752(6) 147 ?
O4 H2 O4 . . 7555 0.89 2.12 2.819(6) 134 ?